Process of producing a phosphoric-acid fertilizer containing urea.



mm m

non. LIE, or mm, nonwnv,

7 1,275,27 No Drawing;

I To all whom it may concern:

' Be it known that I, EGIL Norway, have invented a new and useful Improvement in Processes. of Produclng a.

Phosphoric Acid Fertilizer Containing Urea; and I do hereby declare'the following to baa-full, clear, and

the same. I 1

' The present invention has for its object to provide from-'cy-anamids and acid phos phates a phosphoric acid fertilizer contamingfiirea or its derivatives. I I

It is a"well-known fact that urea may be exact description of I obtained from cyanamids, for instance, from I calcium cyanamid by treatment with acids,

The drawbacks connected with such a proc- I ess are obvious and the process is too expenslve, especially if the urea 1s to be used as a 2o fertilizer.- Thusan excessive quantity of I liquid has to be evaporated, becau'sethe reaction neces'sitatesthe use" of diluted acids.

The present inventionconsists essentially in this that acid phosphate -(either previously prepared or 1n the form of its compo-- nents, whereby the acid phosphate is formed simultaneously with the operations "during which the urea is formed) is treated with cyanamid in the presence of water,

so If the work is carried out in such a man- I ner, the necessity of the evaporation of a large amount of water is avoided and a fer-- tilizer mixture is obtained directly in a state suitable for spreading upon the land. This I as fertilizer, in addition to containing a large its nitrogen in the form of urea,

part of ,contains phosphoric acid in a water-soluble and in a citrate-soluble state, I 1

if, for instance, mono-calcium phosphate 4c is added to calcium cyanamid', the following reactions may take place: I

, Experience has shown that the formation of urea as indicatedrin equation 3'will take place to a considerable degree, if the cond1- tions are maintained which are the most fa Specification of Letters Patent.

4 formation of urea m 'monocalciu'm phosphate.

' Patented A'ugt is, 1918.

Application filed ma e, 1918. Serial No. 282,801.

I I I .the formation of well-known dicyanadi- LIE, citizen'of; Norway, residing at 'Odda, Hardangen.

perature and the time of the treatment.

is avoided. The presence of- Also, it will depend uponthe relative quans tities of cyanamid and phosphate used. In

vcarrying out the-process these conditions are preferably so combined that the greatest" 'possible formation of urea is obtained and:

I at the same time cultl'yj sol ble the formation of" the diifiavoided.

" Even if a surplus of lime-isipresent, in the calcium cyanamid used, only small guantitles of tri-calc ium phosphate will be ormed tri-calcium phosphate is even if stored during a long time at ordi nary temperature.-

This also willbe true, a

if the starting material is dicalcium pho's phateinstead of 'monocalcium phosphate.

- It dicalci'um phosphate, is added to cyanamid, experiencj y be obtained, if water is simultaneously present, withoutjany ,con-

'siderable reformation of tricalcium .phos

phate taln'ng place.

, has shown, that the] 'If an acid phosphate, for instance monocalcium phosphatecontains free phosphoric acid and at least so much calcium'cyanam ld is added as corresponds to the neutralization of the acid, it will be possible to obtain a product containing urea. and also hosphoric acid in the tor-mot a water-so uble larger quantities of cyanamid, the phosphoric acid maybe obtained in a citrate-- tralization of theacid.

If desired, I can treat a mixture of phosphate rock (tri-calcium phosphate) and cal-;

cium cyanamid together with acidand water, to first form the acid phosphate, which then reacts with the -cyanam1d, to produce urea-substances."

calcium phosphate may also bemixed' The acid :By the use of.

er I can add'any kind at I advantageously be used in i with cyanamidand thereafter acid may be. "added. 7

. agaseous state, or instead of the acid its anhydrid maybe used in the presence of the necessary quantity of water.

Incarrying out the process of the invention I can mix the phosphate and oyanamid in any desired proportions, and the percent- 7 ages of nitrogen and phosphoric acid in the product will depend upon the of the two materials used.

According to theinvention T atoid the un- (A) Formation of dicydnaliamioi by at L (B) Formation of urea. Influence of addition of water.

- amas, Mixing proportion. I gggfgfig? f Reaction mlxingtempera- Time. Super I Cyan- Into dic Iu'to I 1 5 31 5; amid. endiamiii. urea.

Perla. Peri. new. d

10 e 1 0 C. 6 30.4 27. 1o 1 1 are. o 11.5 59 10 1 2 are; e 7e .83.

These experiments verify the preceding ones fthe formation of dicyandiamid "being I icons derable if no water is with what. takes together UMGZV and superphosphete.

. The substances are mixed together with out the addition of water or other materials and are allowed to stand without'any regulation of the temperature.

Mixing p p 3 of the nitrogen as dicys h angiamix i upe osa or gg Cyanamad. montha Parts. Part.

10 1 40.8 s 1 50.0 7 1 75.8 5 p 1 419.4 5 V 1 54.7 4 1 58.9

From this is seen that the formation of; dlcyandlamld 1s considerable 1f the two substancesare mixedtogeth'er and are then left free without control.

added compared place if wateris added.

'f The reverse condition is true as regards the formation of urea.

As expected the latter is-increased with the, addition of water;

(G) Formatio rt of urea. Influence of tire temperature. 10 part superphosphateare mixed with l proportions Latest/e part cyanamid and 1 part-Water and the temperatures given below are maintained From this is seen that increasing temperature assists in the formation of'urea.

(D) The retramformation of phosphoric acid.

In this series of tests, 10 parts of superphosphate, 1 part cyanamid and 1 part water were mixed and the mixture held at the temperature indicated below.

' of original ci t ra t e+ water-soluble P 05 citrate-solubie some days after mixing.

Reaction temperature Time.

Hours. 1

The retransformation into insoluble tricalcium phosphate consequently increases 7 with the temperature.

(E) The formation of urea, olicg andiamid and the reversion of P 0 when 80 (or 00 is added to the miwzure of cyanamid and superphosphate. In these experiments the starting material was .a' cyanamidalready containing some dicyandiamid and urea.

Mixing proportion. Some days after mixing %oICaCN,,

. nitrogen I, 7 gr a 21 ea Trainlstforme o r m e 0- 1 P Cyan. d u rin g 75 4 phoe amid Water. the water citrate- .phate. Dieyam soluble. Soluble. diemid. i

Pant. Part9. 10 2 1 15.1 84.9 100. 100.0 3' 1 5 O 18.3 81.7 95.9 lint der I e 1' u q mined 10 4 1 42% 20.8 79.2 93.1 IiOt d0- e r v mined. 10 -5 v 1 32% 25.0 75.0 84.8 100.0

Similar results are produced by the addition fLCO From thisis seen that by the addition of "50 or CO it will be possible to obtain most of the P 01 in a water-soluble state gamma or all P 0 in a citrate-soluble state. At the same time a considerable formation of urea is produced. By combining with those first mentioned at the most favorable temperatures and with the addition of the most favorable amounts of water, it is ossible to obtain most of the nitrogen in the orm of urea with a small amount only of dicyandiamid, and at the same time practically all of the 19 0 is obtained in a watersoluble or a citrate-soluble form.

Consequently, if in agriculture-as it has been proposed-cyanamid and superphosphate are mixed together, one would run the risk of a considerable reversion into insoluble P 0 Besides, considerable quantities of dicyandiamid and smaller quantities of ureaare formed. In such a mixture, when left free without control, the temperature will rise too high and may become uncontrollable; it is obvious that the progress of the reactions taking place is quite uncontrollable. I

Thus although it has heretofore been proposed, to mix superphosphate and calcium cyanamid, the present invention represents novelty being a process of producing a new phosphoric acid fertilizer containing a part of its nitrogen in the form of urea. The feature which is characteristic of the process resides in this that the treatment of acid phosphates is so conducted that formation of urea is caused to take place to a greater or less extent, or-stated 1n another way- 4 a urea containing phosphoric acid fertilizer is produced by treating acid phosphates the last-mentioned method with cyanamid. The means used to solve this problem consists, as explained above, in causing the treatment to take place in presence of water or under influence of water.

While I have referred articularly to the use of calcium cyanami other cyanamid compounds, or cyanamid (H GN can be.

employed. In the appended claims, the expression superphosphate material is intended to cover ready-formed superphosphate or the materials from which it is to be produced.

I claim:

1'. A process of producin a fertilizer containing available phosphorus acid andnitrogen in the'form of urea derivatives, said process comprising mixing a cyanamid, su-

- v EGIL LIE. Witnesses:

N. Gmnson,

Gram BALEL, 

